阅读说明：本技术 一种三七配方颗粒饮片的制备方法 (Preparation method of pseudo-ginseng formula granular decoction pieces ) 是由 杨野 李明 崔秀明 满金辉 王承潇 高明菊 刘迪秋 曲媛 刘源 杨晓燕 熊吟 于 2019-10-22 设计创作，主要内容包括：本发明公开一种三七配方颗粒饮片的制备方法,称取三七原药材,加水煮沸得提取液进行预冻,然后进行真空冷冻干燥,粉碎,过筛；提取物粉末与辅料混匀得到混合物,加入制药用水,超声处理,过滤,收集滤液；滤液预冻,预冻样品采用真空冷冻干燥方式处理；将制备的冻干粉末,加入黏合剂制备软材,制粒、干燥、整粒制备配方颗粒；与传统三七配方颗粒饮片制备工艺相比,本发明制备的颗粒在制备过程中避免了药材提取物因黏度过大,难以和辅料混合均匀的缺点,同时有效降低了产品的吸湿性能和颗粒内部结晶程度,本发明制备的颗粒,延长贮藏时间,同时改善三七药物有效成分在产品中含量的均匀程度,并且其颗粒的色度均一性、流动性都具有显著提高。(The invention discloses a preparation method of pseudo-ginseng formula granule decoction pieces, which comprises the steps of weighing pseudo-ginseng raw medicinal materials, adding water, boiling to obtain an extracting solution, pre-freezing, then carrying out vacuum freeze drying, crushing and sieving; mixing the extract powder with adjuvants to obtain mixture, adding water for preparation, ultrasonic treating, filtering, and collecting filtrate; pre-freezing the filtrate, and treating the pre-frozen sample in a vacuum freeze drying mode; adding the prepared freeze-dried powder into a binding agent to prepare a soft material, and preparing formula granules by granulation, drying and granule finishing; compared with the traditional preparation process of the pseudo-ginseng formula granular decoction pieces, the prepared granules avoid the defects that the medicinal material extract is difficult to be uniformly mixed with auxiliary materials due to overlarge viscosity in the preparation process, and simultaneously effectively reduce the moisture absorption performance of the product and the crystallization degree inside the granules.)

1. A preparation method of pseudo-ginseng formula granular decoction pieces is characterized by comprising the following specific steps:

(1) adding water which is 10 ~ 15 times of the weight of the raw medicinal materials into the raw medicinal materials of the panax notoginseng, boiling for 20-30 minutes to obtain an extracting solution, pre-freezing the obtained extracting solution, then carrying out vacuum freeze drying, crushing and sieving;

(2) and (2) mixing the sieved powder in the step (1) with auxiliary materials according to the mass ratio: auxiliary materials = 1-2: 1, mixing to obtain a mixture, adding pharmaceutical water accounting for 10-20% of the mass of the mixture, carrying out ultrasonic treatment for 20-40 min, filtering, and collecting filtrate;

(3) pre-freezing the filtrate obtained in the step (2);

(4) carrying out vacuum freeze drying on the pre-frozen sample in the step (3);

(5) and (3) adding a binding agent accounting for 10% and ~ 15% of the mass of the freeze-dried powder prepared in the step (4) to prepare a soft material, and then granulating, drying and finishing the soft material to prepare the formula granules.

2. The method for preparing pseudo-ginseng formula particle decoction pieces according to claim 1, wherein the step (1) is carried out by sieving with a sieve of 80 meshes to 120 meshes.

3. The method for preparing pseudo-ginseng formula particle decoction pieces according to claim 1, wherein the adjuvant in the step (2) is lactose, dextrin, soluble starch, mannitol or microcrystalline cellulose.

4. The method for preparing pseudo-ginseng formula granular decoction pieces according to claim 1, wherein the pre-freezing temperature in the step (1) and the step (3) is-30 ℃ to-40 ℃, and the pre-freezing time is 3-5 hours.

5. The method for preparing pseudo-ginseng formula particle decoction pieces according to claim 1, wherein the step (1) and the step (4) of vacuum freeze-drying are carried out under the vacuum degree of 40Pa for 25 hours after the temperature is increased from-35 ℃ to 40 ℃ and then the temperature is kept for 5 hours to 10 hours.

6. The method for preparing pseudo-ginseng granular decoction pieces according to claim 1, wherein the binder in the step (5) is 95% by volume of ethanol or water for pharmacy.

Technical Field

The invention relates to the technical field of pharmaceutical preparation processing, in particular to a method for preparing pseudo-ginseng granular decoction pieces by processing and formulating pseudo-ginseng raw medicinal materials.

Background

Notoginseng [ radix ], [ sic ]Panaxnotoginseng(Burk.)F.H.Chen]Is a perennial herb of araliaceae, is a traditional Chinese medicinal material in China, and is recorded in traditional Chinese medical ancient books such as Ben Cao gang mu and Yu Qi Yao Jie. The notoginseng extract mainly contains notoginseng total saponin, notoginseng extract, flavone, amino acid, saccharide and trace elements, and is the main material of compound red sage dripping pill and Xuesaitong preparation.

The Chinese medicine prescription granule is a granule which is prepared by extracting and concentrating single Chinese medicine decoction pieces and is used for a Chinese medicine clinical prescription, and is mainly characterized in that the granule can replace the traditional Chinese medicine decoction pieces to be used for clinical dialectical treatment of Chinese medical technicians, and simultaneously, decoction is not needed, the concentration of taking after mixing can be automatically adjusted, the volume is small, the application and the carrying are more convenient, and the dissolution and absorption speed is higher. At present, the preparation process of the formula granular decoction pieces refers to a granular preparation, namely, the extract is mixed with a diluent, a binding agent is added to prepare a soft material, and the granular decoction pieces are prepared by a mode of swing granulation or a fluidized bed and the like. According to the formula granules prepared by the method, different production processes not only influence the storage time of the medicine, but also have larger difference in medicine content, and meanwhile, due to the fact that the content of effective components of the medicine in the granules is not uniform due to the preparation process, on one hand, the relative content of traditional Chinese medicinal materials in the product detection is influenced, and on the other hand, the content of the traditional Chinese medicinal materials in each dosage cannot be guaranteed to be consistent during clinical treatment. However, the shelf life of the obtained product is short, and the consistency of the drug content of clinical medication cannot be guaranteed due to the lack of effective measures for uniformly distributing the extract in the granular decoction piece product. Therefore, improving the content uniformity of the effective components of the pseudo-ginseng is an important means for ensuring the clinical application of the pseudo-ginseng formula granule decoction pieces.

Disclosure of Invention

The invention provides a novel preparation method of pseudo-ginseng formula granular decoction pieces, which is characterized in that pseudo-ginseng extract is ground and auxiliary materials are dissolved/mixed in an adhesive, and the principle of ice crystal sublimation is utilized in combination with a vacuum freeze drying mode, so that water in materials is directly sublimated into steam from ice solid without melting ice under a vacuum condition, thereby not only protecting the components which are unstable to heat in pseudo-ginseng medicinal materials, but also enabling the contents of the active ingredients of the pseudo-ginseng medicinal materials in granular products to be more uniform, and ensuring the consistent drug content in clinical application.

The purpose of the invention is realized by the following technical scheme:

a preparation method of pseudo-ginseng formula granular decoction pieces comprises the following specific steps:

(1) adding water which is 10-15 times of the weight of the raw medicinal materials into the raw medicinal materials of pseudo-ginseng, boiling for 20-30 minutes to obtain an extracting solution, pre-freezing the obtained extracting solution, and then carrying out vacuum freeze drying, crushing and sieving on the obtained product;

(2) and (2) mixing the sieved powder in the step (1) with auxiliary materials according to the mass ratio: auxiliary materials = 1-2: 1, mixing to obtain a mixture, adding pharmaceutical water accounting for 10-20% of the mass of the mixture, carrying out ultrasonic treatment for 20-40 min to fully dissolve the mixture, filtering, and collecting filtrate;

(3) pre-freezing the filtrate obtained in the step (2);

(4) processing the pre-frozen sample in the step (3) in a vacuum freeze drying mode;

(5) and (4) adding a binding agent accounting for 10-15% of the mass of the freeze-dried powder prepared in the step (4) to prepare a soft material, and then granulating, drying and finishing to prepare the formula granules.

Sieving the powder with a sieve of 80 meshes to 120 meshes in the step (1).

The auxiliary materials in the step (2) are lactose, dextrin, soluble starch, mannitol or microcrystalline cellulose.

The pre-freezing temperature in the step (1) and the step (3) is-30 to-40 ℃, and the pre-freezing time is 3 to 5 hours.

The vacuum freeze drying in the step (1) and the step (4) is that under the vacuum degree of 40Pa, the temperature is increased from minus 35 ℃ to 40 ℃ for 25 hours, and then the temperature is kept for 5 hours to 10 hours until the temperature is consistent with the temperature of the sample.

Ethanol or pharmaceutical water with the volume fraction of 95 percent in the step (5).

The invention has the beneficial effects that:

(1) the invention utilizes the vacuum freeze drying method to prepare the panax notoginseng extract, can fully protect the active ingredients in the panax notoginseng medicinal material by utilizing the drying principle of low-temperature sublimation, and improves the content of the active ingredients by about 10 percent compared with the traditional drying mode;

(2) the adhesive solution of the pseudo-ginseng extract and the auxiliary material is prepared, so that the pseudo-ginseng extract is fully mixed with the auxiliary material in the solution medium, and the active ingredients of the medicine are distributed more uniformly;

(3) the degree of crystallization in the granules of the pseudo-ginseng formula granular decoction pieces prepared by the invention is improved compared with that of the traditional method;

(4) compared with the traditional preparation process, the equilibrium moisture absorption time of the pseudo-ginseng formula granular decoction pieces prepared by the invention is prolonged by 8% ~ 22%, and the equilibrium moisture absorption amount is reduced by 3% ~ 23%, so that the preservation of the granular decoction pieces is facilitated;

(5) compared with the traditional preparation process of the pseudo-ginseng formula granular decoction pieces, the preparation method disclosed by the invention has the advantages that the defect that the medicinal material extract is difficult to be uniformly mixed with auxiliary materials due to overlarge viscosity is avoided in the preparation process, the hygroscopicity of the product and the crystallization degree inside the granules are effectively reduced, the storage time is prolonged, the content uniformity of the active ingredients of the pseudo-ginseng in the product is improved, and the chroma uniformity and the flowability of the granules are improved.

Drawings

FIG. 1 is an X-ray diffraction pattern of soluble starch, Panax notoginseng root extract, a Panax notoginseng root decoction piece sample prepared in example 1 and a Panax notoginseng root decoction piece sample prepared in comparative example 1;

FIG. 2 is an X-ray diffraction detection of dextrin, Notoginseng radix extract, Notoginseng radix decoction piece sample prepared in example 2 and Notoginseng radix decoction piece sample prepared in comparative example 2;

FIG. 3 is an X-ray diffraction pattern of lactose, Panax notoginseng extract, a Panax notoginseng decoction piece sample prepared in example 3 and a Panax notoginseng decoction piece sample prepared in comparative example 3;

FIG. 4 is an X-ray diffraction pattern of mannitol, a Notoginseng radix extract, a Notoginseng radix decoction piece sample prepared in example 4 and a Notoginseng radix decoction piece sample prepared in comparative example 4;

FIG. 5 is an X-ray diffraction pattern of microcrystalline cellulose, a Panax notoginseng extract, a Panax notoginseng decoction piece sample prepared in example 5 and a Panax notoginseng decoction piece sample prepared in comparative example 5;

fig. 6 is a moisture absorption curve of the pseudo-ginseng formula granule decoction piece samples prepared in examples 1-5 and the pseudo-ginseng formula granule decoction piece samples prepared in comparative examples 1-5, respectively.

Detailed Description

The essential features and the remarkable advantages of the present invention will be further elucidated below by means of examples and figures, without the scope of protection of the invention being limited in any way to the examples.